摘要
匀浆混匀的豆芽样品经磷酸盐缓冲溶液超声提取,提取液经HLB固相萃取小柱净化,甲醇洗脱。采用超高效液相色谱-串联质谱法测定恩诺沙星和环丙沙星的含量,以Agilent Eclipse Plus C18 RRHD色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸-2mmol·L^-1乙酸铵溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。采用同位素内标法定量,恩诺沙星和环丙沙星的线性范围均为0.5~50.0μg·L^-1,检出限(3S/N)均为0.025μg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为89.2%~101%,测定值的相对标准偏差(n=6)为3.3%~9.2%。
The bean sprout sample blended with homogenizer was extracted ultrasonically with phosphate buffer.The extract was purified with HLB solid phase extraction column,and then eluted with methanol.UHPLCMS/MS was applied to the determination of enrofloxacin and ciprofloxacin.Agilent Eclipse Plus C18 RRHD chromatographic column was used as stationary phase,and the mixture of methanol and 0.1%(φ)formic acid-2 mmol·L^-1 ammonium acetate solution mixed in different ratios was used as mobile phase in gradient elution.ESI+and multi-reactions monitor mode were adopted in MS/MS.Isotope was used as internal standard.Linearity ranges of enrofloxacin and ciprofloxacin were both found between 0.5μg·L^-1 and 50.0μg·L^-1,with detection limit(3 S/N)of 0.025μg·kg^-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 89.2%-101%,with RSDs(n=6)of determined values in the range of 3.3%-9.2%.
作者
陈志民
卢军
黄梅英
王华珍
朱丽婷
章舒祺
CHEN Zhimin;LU Jun;HUANG Meiying;WANG Huazhen;ZHU Liling;ZHANG Shuqi(Lishui Bluetown Agricultural Testing Technology Co.,Ltd.,Lishui 323000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第8期927-931,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
